Yin Shi-Jun, Zhou Xi, Peng Li-Jing, Li Fang, Zheng Guo-Can, Yang Feng-Qing, Hu Yuan-Jia
Department of Pharmaceutical Engineering, School of Chemistry and Chemical Engineering, Chongqing University, Chongqing, 401331, China.
Analytical and Testing Center, Chongqing University, Chongqing, 401331, China.
J Pharm Anal. 2022 Aug;12(4):617-626. doi: 10.1016/j.jpha.2022.01.002. Epub 2022 Jan 31.
An innovative sandwich-structural Fe-based metal-organic framework magnetic material (FeO@SW-MIL-101-NH) was fabricated using a facile solvothermal method. The characteristic properties of the material were investigated by field emission scanning electron microscopy, transmission electron microscopy (TEM), energy-dispersive X-ray spectroscopy, Fourier transform infrared spectroscopy, X-ray powder diffraction, vibrating sample magnetometry, and Brunauer-Emmett-Teller measurements. FeO@SW-MIL-101-NH is associated with advantages, such as robust magnetic properties, high specific surface area, and satisfactory storage stability, as well as good selective recognition ability for chlorogenic acid (CA) and its metabolites via chelation, hydrogen bonding, and π-interaction. The results of the static adsorption experiment indicated that FeO@SW-MIL-101-NH possessed a high adsorption capacity toward CA and its isomers, cryptochlorogenic acid (CCA) and neochlorogenic acid (NCA), and the adsorption behaviors were fitted using the Langmuir adsorption isotherm model. Then, a strategy using magnetic solid-phase extraction (MSPE) and ultra-performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry (UPLC-Q-TOF MS/MS) was developed and successfully employed for the selective pre-concentration and rapid identification of CA metabolites in rat plasma, urine, and feces samples. This work presents a prospective strategy for the synthesis of magnetic adsorbents and the high-efficiency pretreatment of CA metabolites.
采用简便的溶剂热法制备了一种创新的三明治结构铁基金属有机框架磁性材料(FeO@SW-MIL-101-NH)。通过场发射扫描电子显微镜、透射电子显微镜(TEM)、能量色散X射线光谱、傅里叶变换红外光谱、X射线粉末衍射、振动样品磁强计和布鲁诺尔-埃米特-泰勒测量等手段对该材料的特性进行了研究。FeO@SW-MIL-101-NH具有诸多优势,如强大的磁性、高比表面积、令人满意的储存稳定性,以及通过螯合、氢键和π相互作用对绿原酸(CA)及其代谢物具有良好的选择性识别能力。静态吸附实验结果表明,FeO@SW-MIL-101-NH对CA及其异构体隐绿原酸(CCA)和新绿原酸(NCA)具有高吸附容量,且吸附行为符合朗缪尔吸附等温线模型。随后,开发了一种利用磁性固相萃取(MSPE)和超高效液相色谱联用四极杆飞行时间串联质谱(UPLC-Q-TOF MS/MS)的策略,并成功用于大鼠血浆、尿液和粪便样品中CA代谢物的选择性预富集和快速鉴定。这项工作为磁性吸附剂的合成以及CA代谢物的高效预处理提供了一种前瞻性策略。